Liu Li-Jun, Luan Qing-Jie, Lu Jing, Lv Dong-Mei, Duan Wen-Zeng, Wang Xu, Gong Shu-Wen
Institute of Functional Organic Molecules and Materials, School of Chemistry and Chemical Engineering, Liaocheng University No. 1 Hunan Road Liaocheng 252000 People's Republic of China
College of Chemistry, Chemical Engineering and Materials Science, Shandong Normal University Jinan 250014 P. R. China.
RSC Adv. 2018 Jul 20;8(46):26180-26187. doi: 10.1039/c8ra04471f. eCollection 2018 Jul 19.
A heteropoly acid based organic hybrid heterogeneous catalyst, HMQ-STW, was prepared by combining 8-hydroxy-2-methylquinoline (HMQ) with Keggin-structured HSiWO (STW). The catalyst was characterized elemental analysis, X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), thermogravimetric analysis (TG) and potentiometric titration analysis. The catalytic performance of the catalyst was assessed in the ketalization of ketones with glycol or 1,2-propylene glycol. Various reaction parameters, such as the glycol to cyclohexanone molar ratio, catalyst dosage, reaction temperature and time, were systematically examined. HMQ-STW exhibited a relatively high yield of corresponding ketal, with 100% selectivity under the optimized reaction conditions. Moreover, catalytic recycling tests demonstrated that the heterogeneous catalyst exhibited high potential for reusability, and it was revealed that the organic modifier HMQ plays an important role in the formation of a heterogeneous system and the improvement of structural stability. These results indicated that the HMQ-STW catalyst is a promising new type of heterogeneous acid catalyst for the ketalization of ketones.
通过将8-羟基-2-甲基喹啉(HMQ)与具有Keggin结构的HSiWO(STW)相结合,制备了一种基于杂多酸的有机杂化多相催化剂HMQ-STW。通过元素分析、X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、热重分析(TG)和电位滴定分析对该催化剂进行了表征。在酮与乙二醇或1,2-丙二醇的缩酮化反应中评估了该催化剂的催化性能。系统研究了各种反应参数,如二醇与环己酮的摩尔比、催化剂用量、反应温度和时间。在优化的反应条件下,HMQ-STW表现出相应缩酮的相对高产率和100%的选择性。此外,催化循环试验表明,该多相催化剂具有很高的可重复使用潜力,并且揭示了有机改性剂HMQ在形成多相体系和提高结构稳定性方面起着重要作用。这些结果表明,HMQ-STW催化剂是一种用于酮缩酮化反应的新型有前途的多相酸催化剂。